A kind of crystal form conversion method of clarithromycin
A technology of clarithromycin and conversion method, which is applied in the field of clarithromycin crystal form conversion, can solve the problems of product loss and large amount of solvents, and achieve the effect of low cost and high efficiency
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Embodiment 1
[0015] step 1: Add 20.0 g (0.0267 mol) of crude clarithromycin and 280 ml of ethanol into a 500 ml four-neck reaction flask equipped with a stirrer and a thermometer, and heat up until the solution becomes clear. After the solution was clarified, the stirring speed was reduced, cooled naturally to room temperature, and then frozen at -10°C for 6h.
[0016] Step 2: The frozen solution is filtered to obtain a clarithromycin wet product, and the crystal form of the wet product is O crystal form. The clarithromycin wet product obtained was rinsed with 500 ml of purified water at room temperature (20° C.), and the crystal form of the wet product was Form II. The yield after drying was 19.6g, and the yield was 98.0%. The X powder diffraction pattern of clarithromycin O crystal form is: 4.599 + 0.2, 6.501 + 0.2, 7.621 + 0.2, 9.196 + 0.2, 10.320 + 0.2, 11.021 + 0.2, 11.763 + 0.2, 11.982 + 0.2, 12.398 + 0.2, 12.638 + 0.2, 13.799 + 0.2, 14.941 + 0.2, 17.098 + 0.2, 18.3...
Embodiment 2
[0018] step 1: It is the same as Step 1 of Embodiment 1.
[0019] Step 2: The frozen solution is filtered to obtain a clarithromycin wet product, and the crystal form of the wet product is O crystal form. The obtained clarithromycin wet product was rinsed with 1000 ml of purified water at room temperature (20° C.). The crystal form of the wet product was Form II, and the yield after drying was 19.5 g, a yield of 97.5%.
Embodiment 3
[0021] step 1: It is the same as Step 1 of Embodiment 1.
[0022] Step 2: The frozen solution is filtered to obtain a clarithromycin wet product, and the crystal form of the wet product is O crystal form. The obtained clarithromycin wet product was rinsed with 200 ml of purified water at 50° C., and the crystal form of the wet product was Form II. The yield after drying was 19.7g, and the yield was 98.5%.
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